HRID2269260

反应详情

EQUATION

反应方程式

HRID 2269260 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of Compound 39 (1.0 g) in acetone (30 ml) was added conc. HCl (4 ml) at room temperature. The reaction mixture was stirred at room temperature for 5 h. The solvent was evaporated in vacuo and the residue was extracted with ether. The combined solution was washed with sat. NaHCO3 aq., and brine, dried(MgSO4) and concentrated in vacuo to give crude product (790 mg) as a yellow solid. The crude product was purified by column chromatography on silica gel with hexane-isopropyl ether(10:1-3:1) to give Compound 40 (275 mg) as a pale yellow solid.

WORKUP

后处理

  1. customThe solvent was evaporated in vacuo
  2. extractionthe residue was extracted with ether
  3. washThe combined solution was washed with sat. NaHCO3 aq., and brine, dried(MgSO4)
  4. concentrationconcentrated in vacuo
  5. customto give crude product (790 mg) as a yellow solid
  6. customThe crude product was purified by column chromatography on silica gel with hexane-isopropyl ether(10:1-3:1)